Dichloromethane → N-(2-Ethoxyethyl)-2-nitroaniline

HRID 2230490

反応式

HRID 2230490 の反応式
Cl[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9].[CH2:11]([O:13][CH2:14][CH2:15][NH2:16])[CH3:12].ClCCl>C(OCC)(=O)C>[CH2:11]([O:13][CH2:14][CH2:15][NH:16][C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][C:3]=1[N+:8]([O-:10])=[O:9])[CH3:12]

参加物

5

反応物 3

HCID 6344DichloromethaneHCID 69451-Chloro-2-nitrobenzeneHCID 66970Ethoxyethylamine

生成物 1

HCID 13623317N-(2-Ethoxyethyl)-2-nitroaniline

試薬・触媒・溶媒 1

HCID 8857Ethyl Acetate溶媒

実験手順

According to the method of R. Iemura et al., J. Med. Chem., 29 1178-1183 (1986), combine 1-chloro-2-nitrobenzene (69.0 g, 440 mmol) and 2-aminoethyl ethyl ether (102.5 g, 1.15 mol) and heat to reflux. After 18 hours, cool and dilute the reaction mixture with ethyl acetate (400 mL). Extract with brine. Dry the organic layer over Na2SO4, filter, and evaporate in vacuo to give a residue. Chromatograph the residue on silica gel eluting with dichloromethane to give N-(2-ethoxyethyl)-2-nitroaniline.

後処理

  1. temperatureheat to reflux
  2. temperaturecool
  3. extractionExtract with brine
  4. dry with materialDry the organic layer over Na2SO4
  5. filtrationfilter
  6. customevaporate in vacuo
  7. customto give a residue

出典と根拠

ORDレコード
ord-2f45f5962851475fb245b68dd965f766
出典データセット
uspto-grants-2002_07
特許番号
US06423704B1

関連ノート

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